HRID1879270

反应详情

EQUATION

反应方程式

HRID 1879270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of compound 112 and 4-bromo-3-methoxyaniline (1 eq.) in DCM (0.15 M) was added PPTS (1 eq.). The mixture was heated to reflux and stirred for one day. The mixture was cooled and the solids were removed by filtration and washed with dichloromethane. The filtrate was concentrated and purified by column chromatography (SiO2, PE:EtOAc with EtOAc from 1 to 15%) to give the title compound 113 (80%). 1H NMR (CDCl3) δ (ppm) 10.32 (br s, 1H), 7.32 (m, 5H), 7.20 (d, J 8.5, 1H), 6.19 (dd, J 8.5, 2.5, 1H), 6.11 (d, J 2.5, 1H), 5.03 (s, 1H), 4.21 (q, J 7.0, 2H), 3.50 (s, 3H), 1.32 (t, J 7.0, 3H).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureThe mixture was cooled
  4. customthe solids were removed by filtration
  5. washwashed with dichloromethane
  6. concentrationThe filtrate was concentrated
  7. custompurified by column chromatography (SiO2, PE:EtOAc with EtOAc from 1 to 15%)